徐 琴,吕 宁,郝鹏飞,孟慧琴,徐 丽,修晓丽,罗 忻.超高效液相色谱-高分辨质谱法快速筛查确证调味品中的19种非食用物质[J].食品安全质量检测学报,2017,8(11):4174-4183
超高效液相色谱-高分辨质谱法快速筛查确证调味品中的19种非食用物质
Screening of 19 kinds of illegal chemical dyes in condiments by ultra performance liquid chromatography-linear ion trap-orbitrap high resolution mass spectrometry
投稿时间:2017-08-04  修订日期:2017-10-26
DOI:
中文关键词:  线性离子阱静电场轨道阱  高分辨质谱  凝胶渗透色谱  调味品  非食用物质
英文关键词:linear ion trap/orbitrap mass spectrometer  high-resolution mass spectrometry  gel permeation chromatography  condiments  illegal chemical dyes
基金项目:
作者单位
徐 琴 山东出入境检验检疫局检验检疫技术中心 
吕 宁 山东出入境检验检疫局检验检疫技术中心 
郝鹏飞 山东出入境检验检疫局检验检疫技术中心 
孟慧琴 山东出入境检验检疫局检验检疫技术中心 
徐 丽 山东出入境检验检疫局检验检疫技术中心 
修晓丽 山东出入境检验检疫局检验检疫技术中心 
罗 忻 山东出入境检验检疫局检验检疫技术中心 
AuthorInstitution
XU Qin Technical Center of Shandong Entry-Exit Inspection and Quarantine Bureau 
LV Ning Technical Center of Shandong Entry-Exit Inspection and Quarantine Bureau 
HAO Peng-Fei Technical Center of Shandong Entry-Exit Inspection and Quarantine Bureau 
MENG Hui-Qin Technical Center of Shandong Entry-Exit Inspection and Quarantine Bureau 
XU Li Technical Center of Shandong Entry-Exit Inspection and Quarantine Bureau 
XIU Xiao-Li Technical Center of Shandong Entry-Exit Inspection and Quarantine Bureau 
LUO Xin Technical Center of Shandong Entry-Exit Inspection and Quarantine Bureau 
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中文摘要:
      目的 建立超高效液相色谱-高分辨质谱法检测调味品中19种非食用物质的分析方法。方法 样品经乙酸乙酯-环己烷提取, 采用凝胶渗透色谱(gel permeation chromatography, GPC)净化与在线定量浓缩, 然后经C18色谱柱分离, 乙腈和5 mmol/L乙酸铵(含0.1%甲酸)溶液梯度洗脱后经超高效液相色谱-线性离子阱/静电场轨道阱高分辨质谱(ultra performance liquid chromatography-linear ion trap-orbitrap high resolution mass spectrometry, UPLC-LTQ-orbitrap MS)测定。结果 19种目标物在15 min内实现良好分离, 线性相关系数均≥0.996, 定量限(limit of quantitation, LOQ)为5~15 μg/kg, 加标回收率在61.9%~105.8%之间, 相对标准偏差(relative standard deviation, RSD)为2.3%~12.9%。结论 本研究建立的方法准确、简单, 可适用于调味品中19种非食用物质的定性定量及确证分析。
英文摘要:
      Objective To establish a method for the determination of 19 kinds of illegal chemical dyes in condiments by the ultra performance liquid chromatography-linear ion trap-orbitrap high resolution mass spectrometry (UPLC-LTQ-Orbitrap MS). Methods The samples were extracted with ethyl acetate-cyclohexane and purified by gel permeation chromatography(GPC) and online quantitative enrichment, and then were separated by the C18 column, and detected by UPLC-LTQ/Orbitrap MS after gradient elution of 5 mmol/L ammonium acetate aqueous solution containing 0.1% formic acid finally. Results Nineteen targets were well separated in 15 min with the correlation coefficients above 0.996, and the limits of quantification (LOD) were 5~15 μg/kg. The recoveries were 61.9%~105.8%, with the relative standard deviations of 2.3%~12.9%. Conclusion The established method is accurate and simple, which can be used in the qualitative and quantitative analysis of 19 kinds of non-edible substances in the condiment.
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